CN109023418A - A kind of preparation method of Pt/ carbon fiber Ti electrode - Google Patents
A kind of preparation method of Pt/ carbon fiber Ti electrode Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
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- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
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- C25B11/055—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material
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- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
- C25B11/093—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds at least one noble metal or noble metal oxide and at least one non-noble metal oxide
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Abstract
The invention discloses a kind of preparation methods of Pt/ carbon fiber Ti electrode, comprising the following steps: step 1, carbon fiber is added in concentrated nitric acid, carbon fiber A is obtained；Step 2, by H2PtCl6·6H2O is dissolved in hydrochloric acid, obtains mixed solution B；Step 3, by NaBH4It is dissolved in water, obtains mixed solution C；Step 4, it takes carbon fiber A to be scattered in mixed solution B, obtains mixed solution D；Step 5, it takes step 3 mixed solution D to mix with mixed solution C, obtains mixed solution E；Step 6, it after mixed solution E filtering, being washed with deionized, is placed in vacuum oven, is dried to after solid powder F mills stand-by；Step 7, the titanium sheet of blasting treatment is boiled in slightly boiled oxalic acid, is saved stand-by in ethanol；Step 8, the solid powder F after milling is taken to mix with polytetrafluoroethylene (PTFE), tabletting, after infrared lamp baking to obtain the final product.This method can be improved electrode catalyst activity, increase electrode life.
Description
Technical field
The invention belongs to be catalyzed the preparation method technical field of Ti electrode, and in particular to a kind of Pt/ carbon fiber Ti electrode
Preparation method.
Background technique
Pt catalyst has good electro catalytic activity, after being prepared into electrode, has been widely used in fuel cell, electricity
The fields such as Xie Shui, supercapacitor.It can be used as the metal oxide containing precious metals of electrochemical catalysis compared to other, Pt catalyst has most
Good electric conductivity and excellent electrocatalysis characteristic, it is non-toxic to humans, it can be applied to electrolysis water ozone field；Compared to electricity
Dizzy method prepares ozone, and there is nitrogenfree oxide to generate, and the excellent characteristic that no poisonous and harmful substance generates has and commercially answers well
With value.
But the Pt catalyst industrially applied causes single Pt catalyst in actual application due at high price at present
In the economic benefit is not high, limit its it is excellent analysis oxygen electrocatalysis characteristic performance.The mode generallyd use now is to utilize activity
Pt catalyst is carried on activated carbon surface, is prepared into Pt/ active carbon by the good electric conductivity of charcoal using active carbon as carrier
Catalyst Ti electrode prepares ozone field using electrolysis water, and reduces the dosage of Pt catalyst, save the cost.
Compared to active carbon, carbon fibre material has more excellent electric conductivity and bigger specific surface area, as novel
Catalyst in carrier, bigger effect will be played.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods of Pt/ carbon fiber Ti electrode, can be improved electrode catalyst activity,
Increase electrode life.
The technical scheme adopted by the invention is that a kind of preparation method of Pt/ carbon fiber Ti electrode, comprising the following steps:
Step 1, carbon fiber is added in 98% concentrated nitric acid of mass fraction, is flowed back, then with deionized water dilute solution
To neutrality, centrifugation, washing are subsequently placed to drying in baking oven, obtain carbon fiber A of the surface by modification；
Step 2, by H2PtCl6·6H2O is dissolved in the hydrochloric acid that mass fraction is 5%, obtains being the mixed of 0.1g/l containing Pt
Close solution B；
Step 3, by NaBH4Dissolution in deionized water, obtains NaBH4For the mixed solution C of 37g/l；
Step 4, then, take carbon fiber A to be scattered in mixed solution B, be configured to Pt and carbon fiber A mass ratio is 1:200
The mixed solution of~1:2, ultrasonic disperse obtain mixed solution D；
Step 5, step 3 mixed solution D is taken to mix with mixed solution C, the volume that mixed solution D is mixed with mixed solution C
Than obtaining mixed solution E for 1:0.5~1:2, ultrasonic 10min；
Step 6, it after mixed solution E filtering, being washed with deionized, is placed in vacuum oven, 5 hours, 150
DEG C, it is dried to after solid powder F mills stand-by；
It step 7, is to boil 1~2h in 10~15% oxalic acid solutions in slightly boiled mass fraction by the titanium sheet of blasting treatment,
It performs etching, is rinsed after the completion of etching with a large amount of deionized waters, then saved stand-by in ethanol；
Step 8, the solid powder F after milling is taken to mix with polytetrafluoroethylene (PTFE), solid powder F is dense in polytetrafluoroethylene (PTFE)
Degree is 0.1g/l~1g/l, and Pt/ carbon fiber Ti electrode is made after infrared lamp baking with the titanium sheet adhesion in step 7 in tabletting.
The features of the present invention also characterized in that
Carbon fiber outer diameter is 7 μm.
In step 1, flow back 5h under conditions of 160 DEG C, is placed in 60 DEG C of baking ovens sufficiently dry.
In step 4,30~60min of ultrasonic disperse obtains solution D.
In step 8, the time of infrared lamp baking is 10min.
The beneficial effects of the present invention are: the method for the present invention disperses the carbon fiber of acidification in the acid solution of Pt, so
The dispersion liquid and NaBH will be contained afterwards4Solution mixing, Pt is directly reduced to atomic state and is carried on carbon fiber surface, then by this
After mixed solution filtration washing, vacuum drying is milled into powder.Tabletting is in titanium sheet table after powder is mixed with polytetrafluoroethylene (PTFE) again
Pt/ carbon fiber Ti electrode is made in face.Compared to traditional Pt/ active carbon Ti electrode, reinforcing life increases 15~20% left sides
The right side improves its economic benefit, promotes electrolysis method and prepares ozone in the wider application of sterilizing industry；And entire system
Standby process is easy to operate, and may be implemented to produce in batches.
Specific implementation
The present invention is described in detail With reference to embodiment.
The present invention provides a kind of preparation methods of Pt/ carbon fiber Ti electrode, comprising the following steps:
Step 1, carbon fiber is added in 98% concentrated nitric acid of mass fraction, flow back 5h under conditions of 160 DEG C, then with
Deionized water dilute solution to neutrality, centrifugation, washing is placed in 60 DEG C of baking ovens and sufficiently dries, and obtains surface by modification
Carbon fiber A；Wherein, carbon fiber outer diameter is 7 μm；In step 1；
Step 2, by H2PtCl6·6H2O is dissolved in the hydrochloric acid that mass fraction is 5%, obtains being the mixed of 0.1g/l containing Pt
Close solution B；
Step 3, by NaBH4Dissolution in deionized water, obtains NaBH4For the mixed solution C of 37g/l；
Step 4, then, take carbon fiber A to be scattered in mixed solution B, be configured to Pt and carbon fiber A mass ratio is 1:200
The mixed solution of~1:2,30~60min of ultrasonic disperse obtain mixed solution D；
Step 5, step 3 mixed solution D is taken to mix with mixed solution C, the volume that mixed solution D is mixed with mixed solution C
Than obtaining mixed solution E for 1:0.5~1:2, ultrasonic 10min；
Step 6, it after mixed solution E filtering, being washed with deionized, is placed in vacuum oven, 5 hours, 150
DEG C, it is dried to after solid powder F mills stand-by；
It step 7, is to boil 1~2h in 10~15% oxalic acid solutions in slightly boiled mass fraction by the titanium sheet of blasting treatment,
It performs etching, is rinsed after the completion of etching with deionized water, then saved stand-by in ethanol；
Step 8, the solid powder F after milling is taken to mix with polytetrafluoroethylene (PTFE), solid powder F is dense in polytetrafluoroethylene (PTFE)
Degree is 0.1g/l~1g/l, and tabletting, with the titanium sheet adhesion in step 7, Pt/ carbon fiber titanium is made after toasting 10min in infrared lamp
Electrode.
Embodiment 1:
3g carbon fiber is added in 98% concentrated nitric acid of 500ml mass fraction, 160 DEG C of reflux are then dilute with deionized water
Solution is released to neutrality, centrifugation, washing are subsequently placed to 60 DEG C of dry 6h in baking oven, obtain carbon fiber A of the surface by modification；
By H2PtCl6·6H2O is dissolved in the hydrochloric acid that mass fraction is 5%, obtains the mixed solution B of Pt 0.1g/l；By 37g NaBH4
It is dissolved in 1l deionized water, obtains NaBH4For the mixed solution C of 37g/l；By the titanium sheet (30mm* of 50 mesh blasting treatments
It is 30mm*1.5mm) to boil 1~2h in 10~15% oxalic acid solutions in slightly boiled mass fraction, performs etching, used after the completion of etching
A large amount of deionized waters are rinsed, and are then saved stand-by in ethanol；
It takes 100mg carbon fiber A to be scattered in 30ml mixed solution B, is configured to Pt and carbon fiber mass ratio is the mixed of 3:100
Solution is closed, ultrasonic disperse obtains mixed solution D；50 μ l of mixed solution D is mixed with 50ul mixed solution C, and the two volume ratio is 1:
1, ultrasonic 10min obtain mixed solution E；Mixed solution E is filtered, is washed with deionized to neutrality, it is dry to be placed in vacuum
In dry case, 5 hours, 150 DEG C, it is dried to after solid powder F mills stand-by.Take the solid powder F 0.83g after milling and 1ml poly-
After tetrafluoroethene is stirred, concentration 0.83g/l, tabletting, and the titanium sheet adhesion handled well, infrared lamp toasted after 10min i.e.
Pt/ carbon fiber Ti electrode is made.
Using the electrode as cathode, brown lead oxide is as anode, is electrolysis with pure water using Nafion117 as diaphragm
Matter, current density 3500A/m2, ozone yield is 6mmol/l.With 0.5mol/LH2SO4Solution is electrolyte, with
20000A/m2Current density it is electrolysed, measure tank voltage increase 4V when service life be about 300h.
Embodiment 2:
3g carbon fiber is added in 98% concentrated nitric acid of 500ml mass fraction, 160 DEG C of reflux are then dilute with deionized water
Solution is released to neutrality, centrifugation, washing are subsequently placed to 60 DEG C of dry 6h in baking oven, obtain carbon fiber A of the surface by modification；
By H2PtCl6·6H2O is dissolved in the hydrochloric acid that mass fraction is 5%, obtains the mixed solution B of Pt 0.1g/l；By 37g NaBH4
It is dissolved in 1l deionized water, obtains NaBH4For the mixed solution C of 37g/l；By the titanium sheet (30mm* of 50 mesh blasting treatments
It is 30mm*1.5mm) to boil 1~2h in 10~15% oxalic acid solutions in slightly boiled mass fraction, performs etching, used after the completion of etching
A large amount of deionized waters are rinsed, and are then saved stand-by in ethanol；
It takes 100mg carbon fiber A to be scattered in 50ml mixed solution B, is configured to Pt and carbon fiber mass ratio is the mixed of 5:100
Solution is closed, ultrasonic disperse obtains mixed solution D；50 μ l of mixed solution D is mixed with 25ul mixed solution C, and the two volume ratio is 1:
0.5, ultrasonic 10min obtain mixed solution E；Mixed solution E is filtered, is washed with deionized to neutrality, vacuum is placed in
In drying box, 5 hours, 150 DEG C, it is dried to after solid powder F mills stand-by.Take solid powder F 0.5g and 1ml after milling
After Teflon stir mixing, concentration 0.5g/l, tabletting, and the titanium sheet adhesion handled well, infrared lamp toasted after 10min i.e.
Pt/ carbon fiber Ti electrode is made.
Using the electrode as cathode, brown lead oxide is as anode, is electrolysis with pure water using Nafion117 as diaphragm
Matter, current density 3500A/m2, ozone yield is 8.2mmol/l.With 0.5mol/LH2SO4Solution is electrolyte, with
20000A/m2Current density it is electrolysed, measure tank voltage increase 4V when service life be about 331h.
Embodiment 3:
3g carbon fiber is added in 98% concentrated nitric acid of 500ml mass fraction, 160 DEG C of reflux are then dilute with deionized water
Solution is released to neutrality, centrifugation, washing are subsequently placed to 60 DEG C of dry 6h in baking oven, obtain carbon fiber A of the surface by modification；
By H2PtCl6·6H2O is dissolved in the hydrochloric acid that mass fraction is 5%, obtains the mixed solution B of Pt 0.1g/l；By 37g NaBH4
It is dissolved in 1l deionized water, obtains NaBH4For the mixed solution C of 37g/l；By the titanium sheet (30mm* of 50 mesh blasting treatments
It is 30mm*1.5mm) to boil 1~2h in 10~15% oxalic acid solutions in slightly boiled mass fraction, performs etching, used after the completion of etching
A large amount of deionized waters are rinsed, and are then saved stand-by in ethanol；
It takes 50mg carbon fiber A to be scattered in 50ml mixed solution B, is configured to Pt and carbon fiber mass ratio is the mixed of 10:100
Solution is closed, ultrasonic disperse obtains mixed solution D；50 μ l of mixed solution D is mixed with 40ul mixed solution C, and the two volume ratio is 1:
0.8, ultrasonic 10min obtain mixed solution E；Mixed solution E is filtered, is washed with deionized to neutrality, vacuum is placed in
In drying box, 5 hours, 150 DEG C, it is dried to after solid powder F mills stand-by.Take solid powder F 0.25g and 1ml after milling
After Teflon stir mixing, concentration 0.25g/l, tabletting, and the titanium sheet adhesion handled well, after infrared lamp toasts 10min
Pt/ carbon fiber Ti electrode is made.
Using the electrode as cathode, brown lead oxide is as anode, is electrolysis with pure water using Nafion117 as diaphragm
Matter, current density 3500A/m2, ozone yield is 7.6mmol/l.With 0.5mol/L H2SO4Solution is electrolyte, with
20000A/m2Current density it is electrolysed, measure tank voltage increase 4V when service life be about 268h.
Embodiment 4:
3g carbon fiber is added in 98% concentrated nitric acid of 500ml mass fraction, 160 DEG C of reflux are then dilute with deionized water
Solution is released to neutrality, centrifugation, washing are subsequently placed to 60 DEG C of dry 6h in baking oven, obtain carbon fiber A of the surface by modification；
By H2PtCl6·6H2O is dissolved in the hydrochloric acid that mass fraction is 5%, obtains the mixed solution B of Pt 0.1g/l；By 37g NaBH4
It is dissolved in 1l deionized water, obtains NaBH4For the mixed solution C of 37g/l；By the titanium sheet (30mm* of 50 mesh blasting treatments
It is 30mm*1.5mm) to boil 1~2h in 10~15% oxalic acid solutions in slightly boiled mass fraction, performs etching, used after the completion of etching
A large amount of deionized waters are rinsed, and are then saved stand-by in ethanol；
It takes 10mg carbon fiber A to be scattered in 50ml mixed solution B, is configured to Pt and carbon fiber mass ratio is the mixed of 50:100
Solution is closed, ultrasonic disperse obtains mixed solution D；50 μ l of mixed solution D is mixed with 50ul mixed solution C, and the two volume ratio is 1:
1, ultrasonic 10min obtain mixed solution E；Mixed solution E is filtered, is washed with deionized to neutrality, it is dry to be placed in vacuum
In dry case, 5 hours, 150 DEG C, it is dried to after solid powder F mills stand-by.Take the solid powder F 0.1g after milling and 1ml poly-
After tetrafluoroethene is stirred, concentration 0.1g/l, tabletting, with the titanium sheet adhesion handled well, infrared lamp is made after toasting 10min
At Pt/ carbon fiber Ti electrode.
Using the electrode as cathode, brown lead oxide is as anode, is electrolysis with pure water using Nafion117 as diaphragm
Matter, current density 3500A/m2, ozone yield is 6.4mmol/l.With 0.5mol/LH2SO4Solution is electrolyte, with
20000A/m2Current density it is electrolysed, measure tank voltage increase 4V when service life be about 264h.
Embodiment 5:
3g carbon fiber is added in 98% concentrated nitric acid of 500ml mass fraction, 160 DEG C of reflux are then dilute with deionized water
Solution is released to neutrality, centrifugation, washing are subsequently placed to 60 DEG C of dry 6h in baking oven, obtain carbon fiber A of the surface by modification；
By H2PtCl6·6H2O is dissolved in the hydrochloric acid that mass fraction is 5%, obtains the mixed solution B of Pt 0.1g/l；By 37g NaBH4
It is dissolved in 1l deionized water, obtains NaBH4For the mixed solution C of 37g/l；By the titanium sheet (30mm* of 50 mesh blasting treatments
It is 30mm*1.5mm) to boil 1~2h in 10~15% oxalic acid solutions in slightly boiled mass fraction, performs etching, used after the completion of etching
A large amount of deionized waters are rinsed, and are then saved stand-by in ethanol；
It takes 1000mg carbon fiber A to be scattered in 50ml mixed solution B, is configured to Pt and carbon fiber mass ratio is 1:200's
Mixed solution, ultrasonic disperse obtain mixed solution D；50 μ l of mixed solution D is mixed with 100ul mixed solution C, and the two volume ratio is
1:2, ultrasonic 10min obtain mixed solution E；Mixed solution E is filtered, is washed with deionized to neutrality, vacuum is placed in
In drying box, 5 hours, 150 DEG C, it is dried to after solid powder F mills stand-by.Take the solid powder F 1g after milling and 1ml poly-
After tetrafluoroethene is stirred, concentration is 1g/l tabletting, and with the titanium sheet adhesion handled well, infrared lamp is made after toasting 10min
Pt/ carbon fiber Ti electrode.
Using the electrode as cathode, brown lead oxide is as anode, is electrolysis with pure water using Nafion117 as diaphragm
Matter, current density 3500A/m2, ozone yield is 5.2mmol/l.With 0.5mol/LH2SO4Solution is electrolyte, with
20000A/m2Current density it is electrolysed, measure tank voltage increase 4V when service life be about 245h.
From in above embodiments 1-5 as can be seen that present invention utilizes Pt catalyst electrolysis water reaction in good electricity
Catalytic activity, has prepared Pt/ carbon fiber Ti electrode, which has the service life long, the characteristics of to the less pollution of environment, because
This, this method is a kind of raising water electrolytic ozone yield, increases electrode life, reduces the good electrolysis water system of electrode cost
The preparation method of ozone electrode.
Claims (5)
1. a kind of preparation method of Pt/ carbon fiber Ti electrode, which comprises the following steps:
Step 1, carbon fiber is added in 98% concentrated nitric acid of mass fraction, is flowed back, then with deionized water dilute solution into
Property, centrifugation, washing are subsequently placed to drying in baking oven, obtain carbon fiber A of the surface by modification；
Step 2, by H2PtCl6·6H2O is dissolved in the hydrochloric acid that mass fraction is 5%, is obtained molten containing the mixing that Pt is 0.1g/l
Liquid B；
Step 3, by NaBH4Dissolution in deionized water, obtains NaBH4For the mixed solution C of 37g/l；
Step 4, then, take carbon fiber A to be scattered in mixed solution B, be configured to Pt and carbon fiber A mass ratio is 1:200~1:2
Mixed solution, ultrasonic disperse obtains mixed solution D；
Step 5, step 3 mixed solution D is taken to mix with mixed solution C, the volume ratio that mixed solution D is mixed with mixed solution C is
1:0.5~1:2, ultrasonic 10min obtain mixed solution E；
Step 6, it after mixed solution E filtering, being washed with deionized, is placed in vacuum oven, 5 hours, 150 DEG C, does
It is dry mill at solid powder F after it is stand-by；
Step 7, it is to boil 1~2h in 10~15% oxalic acid solutions in slightly boiled mass fraction by the titanium sheet of blasting treatment, carries out
It etches, is rinsed after the completion of etching with deionized water, then saved stand-by in ethanol；
Step 8, the solid powder F after milling is taken to mix with polytetrafluoroethylene (PTFE), concentration of the solid powder F in polytetrafluoroethylene (PTFE) is
Pt/ carbon fiber Ti electrode is made after infrared lamp baking with the titanium sheet adhesion in step 7 in 0.1g/l~1g/l, tabletting.
2. a kind of preparation method of Pt/ carbon fiber Ti electrode according to claim 1, which is characterized in that the carbon fiber
Outer diameter is 7 μm.
3. a kind of preparation method of Pt/ carbon fiber Ti electrode according to claim 1, which is characterized in that the step 1
In, flow back 5h under conditions of 160 DEG C, is placed in 60 DEG C of baking ovens sufficiently dry.
4. a kind of preparation method of Pt/ carbon fiber Ti electrode according to claim 1, which is characterized in that the step 4
In, 30~60min of ultrasonic disperse obtains solution D.
5. a kind of preparation method of Pt/ carbon fiber Ti electrode according to claim 1, which is characterized in that the step 8
In, the time of infrared lamp baking is 10min.
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